US3909439A - Process for the production of aluminum chlorohydroxides - Google Patents
Process for the production of aluminum chlorohydroxides Download PDFInfo
- Publication number
- US3909439A US3909439A US336753A US33675373A US3909439A US 3909439 A US3909439 A US 3909439A US 336753 A US336753 A US 336753A US 33675373 A US33675373 A US 33675373A US 3909439 A US3909439 A US 3909439A
- Authority
- US
- United States
- Prior art keywords
- range
- aluminum
- hydrochloric acid
- amount
- formula
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q15/00—Anti-perspirants or body deodorants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/26—Aluminium; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/22—Halogenating
- B01J37/24—Chlorinating
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
Definitions
- the present invention relates to a process for the production of aluminum chlorohydroxides.
- the present invention relates to a process for the production of aluminium chlorohydroxides having the general formula Al (Ol-1),,.Cl,, wherein x and y may range from 1 to 3.5 and from 5 to 2.5 respectively.
- alumina Bayer bauxite, bayerite, gibbsite, hydrargillit, diaspore, boemite of as to the more common types, but it is possible to use, as starting material, any aluminum oxide or hydroxide.
- the inventive process consistis in attacking the starting material with hydrochloric acid, in an amount which is from (lto 1/4)/2.5) the stoichiometric amount for obtaining the trichloride.
- the reaction occurs at temperatures ranging from 100 to 160C, and at pressures ranging from 0.1 kg/cm to 4 kg/cm and is completed after 2 to 10 hours from the beginning.
- a part of alumina added in excess does not react and remains as a solid residue, which can be removed and fed again to the etching reactor. Its reactivity is quite similar to the one of the product originally fed.
- the employed aluminas can possess particles of various size.
- the chlorohydroxides obtained according to the inventive process may be employed as follows: preparation of 'y-alumina as an active basis of catalysts, mordanting textile fibers, in the cosmetics industry as, for instance, in antisudorific powders.
- EXAMPLE 1 Use was made of alumina Bayer, having particles with a 40 70 u diameter, (A1 3 H 0) and the following nominal composition (by weight):
- the reaction was performed with kg of H Cl in a Pyrex glass or enameled steel reactor at a temperature ranging between C and C, the reactor being kept under an inert gas atmosphere of from 0.8 to 1.5 kg/cm and a strong mechanical stirring.
- the suspension was diluted with 25 liters of distilled water containing 100 g of H Cl (d 1.19), discharged from reactor and centrifuged by means of a basket centrifuge of lncoloy 825 after cooling at a temperature ranging from 50 to 85C, by means of a heat exchanger in lncoloy 825.
- composition, pH and the density of the chlorohydroxide obtained from the etching, after the removal of the solid residue were the following ones:
- the weight ratio between A1 and Cl is 0.46 0.54, which corresponds to an approximate composition of Al (0l1-1) Cl EXAMPLE 2
- the etching was performed by employing 100 kg of Alumina Bayer and 179 kg of H Cl (d 32 1.19), at a temperature of 110C, for a reaction time of 8 hours and at a pressure of 0.5 kg/cm
- the analysis of the obtained product showed the composition as:
Abstract
Aluminum chlorohydroxide represented by the formula: Al2(OH)x Cly, wherein x and y range from 1 to 3.5 and 5 to 2.5, respectively, is produced by reacting aluminum oxide or hydroxide with an amount of hydrochloric acid which is (1/2.5) to (1/4) of the stoichiometric amount for obtaining aluminum trichloride, at a temperature in the range from 100*C to 160*C, and at a pressure in the range from 0.1 kg/cm2 to 4 kg/cm2 for a period of from 2 to 10 hours.
Description
United States Patent 11 1 Rivola et al.
1451 Sept. 30, 1975 PROCESS FOR THE PRODUCTION OF ALUMINUM CHLOROHYDROXIDES [75] Inventors: Luigi Rivola; Bruno Notari, both of San Donato Milanese, Italy [73] Assignee: Snam Progetti S.p.A., San Donato Milanese, Italy [22] Filed: Feb. 28, 1973 [21] Appl. No.: 336,753
[30] Foreign Application Priority Data Mar. 1, 1972 Italy 21252/72 [52] US. Cl 252/187 R; 423/472; 423/127 [5]] Int. Cl.' COIF 7/00; COlF 7/22;CO1F 7/56 [58] Field of Search 252/187 R; 423/462, 127,
[56] References Cited UNITED STATES PATENTS 12/1963 Jones 204/252 Primary Examiner-Benjamin R. Padgett Assistant ExaminerB. Hunt Attorney, Agent, or FirmRalph M. Watson, Esq.
[ 5 7] ABSTRACT 2 Claims, No lDrawings PROCESS FOR THE PRODUCTION OF ALUMHNUM CHLOROHYDROXIDES The present invention relates to a process for the production of aluminum chlorohydroxides.
More particularly the present invention relates to a process for the production of aluminium chlorohydroxides having the general formula Al (Ol-1),,.Cl,, wherein x and y may range from 1 to 3.5 and from 5 to 2.5 respectively.
It is known that alumina is attacked by hydrochloric acid, and the reaction gives rise to aluminum trichloride, particularly when the amount of hydrochloric acid employed is higher than the stoichiometric one.
It has now been found that, by employing an amount of aluminum oxide or hydroxide in excess of the stoichiometric one necessary for obtaining the trichloride the reaction proceeds to the formation of chlorohydroxides having the above formula under appropriate working conditions.
According to the process of the present invention use may be made of alumina Bayer, bauxite, bayerite, gibbsite, hydrargillit, diaspore, boemite of as to the more common types, but it is possible to use, as starting material, any aluminum oxide or hydroxide.
The inventive process consistis in attacking the starting material with hydrochloric acid, in an amount which is from (lto 1/4)/2.5) the stoichiometric amount for obtaining the trichloride.
The reaction occurs at temperatures ranging from 100 to 160C, and at pressures ranging from 0.1 kg/cm to 4 kg/cm and is completed after 2 to 10 hours from the beginning.
A part of alumina added in excess does not react and remains as a solid residue, which can be removed and fed again to the etching reactor. Its reactivity is quite similar to the one of the product originally fed.
The employed aluminas can possess particles of various size.
Particular advantages have been realized by using products with particles having 500 1,000 A diameter. However the preparation of oxides and hydroxides having such small sizes is not convenient from an economical point of view. Therefore, materials with sizes ranging from a few microns to a few hundred microns are also employable in the process described.
The chlorohydroxides obtained according to the inventive process may be employed as follows: preparation of 'y-alumina as an active basis of catalysts, mordanting textile fibers, in the cosmetics industry as, for instance, in antisudorific powders.
The inventive process will be better understood through consideration of the following illustrative examples.
EXAMPLE 1 Use was made of alumina Bayer, having particles with a 40 70 u diameter, (A1 3 H 0) and the following nominal composition (by weight):
Ano, 64.9 65.1 "/1 Total Na O 0.4 Soluble Na O 0.045 s1 0.009 Fe 0.012 Ti 0.003 P 0.001 a v 0.000% 14,0 at 110C 0.1 [-120 at 1000a: 35.0
Alumina Bayer was attacked with an aquous solution of hydrochloric acid at 37 (zi= 1.19).
The reaction was performed with kg of H Cl in a Pyrex glass or enameled steel reactor at a temperature ranging between C and C, the reactor being kept under an inert gas atmosphere of from 0.8 to 1.5 kg/cm and a strong mechanical stirring.
After 4 hours run, the suspension was diluted with 25 liters of distilled water containing 100 g of H Cl (d 1.19), discharged from reactor and centrifuged by means of a basket centrifuge of lncoloy 825 after cooling at a temperature ranging from 50 to 85C, by means of a heat exchanger in lncoloy 825.
Following the etching 50 of Alumina Bayer charged into the reactor 50 kg) is solubilized. Therefore the solid residue from the centrifuge was put again in the etching reactor, and the starting amount was restored with 50 kg of fresh Alumina Bayer. 100 kg ofH Cl (d== 1.19) were again added to the reactor and the etching was again carried out as described above.
The composition, pH and the density of the chlorohydroxide obtained from the etching, after the removal of the solid residue, were the following ones:
A1 0 19.5 20.5 (by weight) Cl 21.0 22.0 (by weight) Fe 80 p.p.m.
Na 13.50 ppm.
pH 20C 085 1.00
The weight ratio between A1 and Cl is 0.46 0.54, which corresponds to an approximate composition of Al (0l1-1) Cl EXAMPLE 2 According to the preceding example and with the same starting material, the etching was performed by employing 100 kg of Alumina Bayer and 179 kg of H Cl (d 32 1.19), at a temperature of 110C, for a reaction time of 8 hours and at a pressure of 0.5 kg/cm The analysis of the obtained product showed the composition as:
17-18% ZZZ-24% The approximate formula of obtained chlorohydroxide was Al (Ol-{) Cl The unreacted residue, lying on the reactor bottom, was 10 15 with respect to the starting amount fed to the reactor.
What we claim is:
l. The process of producing aluminum chlorohydroxide represented by the formula: Al OH) Cl wherein x and y range from 1 to 3.5 and from 5 to 2.5, respectively, which consists of reacting aluminum oxide or hydroxide with an amount of hydrochloric acid which is from (V2.5) to (H4) of the stoichiometric amount for obtaining aluminum trichloride, at a temperature in the range from 100C to C, and at a pressure in the range from 0.1 kg/cm to 4 kg/cm for a period of from 2 to 10 hours.
2. The process of producing aluminum chlorohydroxide represented by the formula: Al (OH) Cl wherein x and y range from 1 to 3.5 and from 5 to 2.5, respectively, as claimed in claim 1, in which the hydrochloric acid is caused to react with a member of the group consisting of: alumina Bayer, bauxite, bayerite, gibbsite, hydrargillite, diaspore and boehmite.
UNITED STATES PATENT AND TRADEMARK OFFICE CERTIFICATE OF CORRECTION PATENT N0. DATED lNV ENTOR(S) 3,909,439 T September 30, 1975 Luigi Rivola and Bruno Notari His certified that error appears in the above-identified patent and thatsaid Letters Patent are hereby corrected as shown below:
Abstract, line 5, "(l/2.5) to (1/4)" should read Column 1, line line line Column 2, line line [SEAL] --l/Z.5 to 1/4 of-.
"(d 32 1/19) should read -(d=l.1.9)--.
"(l/2.5) to (1/4)" should read l/2.5 to l/4.
Signed and Scaled this eighteenth Day of May 1976 Arlen.-
RUTH c. MASON. Alluring Officer 'C. MARSHALL DANN Commissioner oflalenrs and Trademark-x UNITED STATES PATENT AND TRADEMARK OFFICE CERTIFICATE OF CORRECTION PATENT NO.
DATED INVENTOR(S) 3,909,439 September 30, 1975 Luigi Rivola and Bruno Notari It is certified that error appears in the ab0ve-identified patent and that said Letters Patent are hereby corrected as shown below:
Abstract, line Column 1, line line line
Column 2, line line [SEAL] 5, "(l/2.5) to (1/4)" should read --l/2.5 to 1/4".
4, "aluminium" should read --aluminum--.
22, "as to" should be deleted.
27, "(l to l/4)/2.5)" should read --l/2.5 to 1/4.
I Signed and Scaled this eighteenth Day of May 1976 A nest:
RUTH c. msou Arresting Officer 'C. MARSHALL DANN (ommissiunvr nj'lamm and Tradvmarkx
Claims (2)
1. THE PROCESS OF PRODUCING ALUMINUM CHLOROHYDROXIDE REPRESENTED BY THE FORMULA: A12(OH)XCLY, WHEREIN X AND Y RANGE FROM 1 TO 3.5 AND FROM 5 TO 2.5, RESPECTIVELY, WHICH CONSISTS OF REACTING ALUMINUM OXIDE OR HYDROXIDE WITH AN AMOUNT OF HYDROCHLORIC ACID WHICH IS FROM (1/2.5E TO (1/4) OF THE STOICHIOMETRIC AMOUNT FOR OBTAINING ALUMINUM TRICHLORIDE, AT A TEMPERATURE IN THE RANGE FROM 100*C TO 160*, AND AT A PRESSURE IN THE RANGE FROM 0.1 KG/CM2 TO 4 KG/CM2 FOR A PERIOD OF FROM 2 TO 10 HOURS.
2. The process of producing aluminum chlorohydroxide represented by the formula: Al2(OH)xCly, wherein x and y range from 1 to 3.5 and from 5 to 2.5, respectively, as claimed in claim 1, in which the hydrochloric acid is caused to react with a member of the group consisting of: alumina Bayer, bauxite, bayerite, gibbsite, hydrargillite, diaspore and boehmite.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IT21252/72A IT949756B (en) | 1972-03-01 | 1972-03-01 | PROCESS FOR THE PRODUCTION OF ALUMINUM CHLOROHYDROXIDES |
Publications (1)
Publication Number | Publication Date |
---|---|
US3909439A true US3909439A (en) | 1975-09-30 |
Family
ID=11179064
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US336753A Expired - Lifetime US3909439A (en) | 1972-03-01 | 1973-02-28 | Process for the production of aluminum chlorohydroxides |
Country Status (28)
Country | Link |
---|---|
US (1) | US3909439A (en) |
JP (1) | JPS48101399A (en) |
AR (1) | AR201100A1 (en) |
AT (1) | AT329520B (en) |
AU (1) | AU475570B2 (en) |
BE (1) | BE795923A (en) |
CA (1) | CA1005969A (en) |
CH (1) | CH560163A5 (en) |
CS (1) | CS184813B2 (en) |
DD (1) | DD102370A5 (en) |
DE (1) | DE2310014C2 (en) |
DK (1) | DK143063C (en) |
ES (1) | ES412423A1 (en) |
FR (1) | FR2174114B1 (en) |
GB (1) | GB1410087A (en) |
HU (1) | HU165434B (en) |
IE (1) | IE37607B1 (en) |
IN (1) | IN138595B (en) |
IT (1) | IT949756B (en) |
LU (1) | LU67122A1 (en) |
NL (1) | NL7302847A (en) |
NO (1) | NO131641C (en) |
RO (1) | RO64459A (en) |
SE (1) | SE388191B (en) |
TR (1) | TR17931A (en) |
YU (1) | YU36664B (en) |
ZA (1) | ZA731255B (en) |
ZM (1) | ZM3273A1 (en) |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4082685A (en) * | 1974-03-28 | 1978-04-04 | Snamprogetti, S.P.A. | Process for the production of aluminum chlorohydroxides |
US5120522A (en) * | 1989-01-25 | 1992-06-09 | Caffaro S.P.A. | Process for preparing basic aluminum compounds |
US5182094A (en) * | 1989-02-13 | 1993-01-26 | Kemira Kemi Aktiebolag | Process for the preparation of polyaluminum compounds |
EP0554562A1 (en) * | 1992-02-01 | 1993-08-11 | A.I.R. Lippewerk Recycling GmbH | Process for the preparation of basic aluminium chloride solutions |
US5830388A (en) * | 1995-08-11 | 1998-11-03 | American Envirocare, Inc. | Coagulating and flocculating agent and method for making it |
US5985234A (en) * | 1995-09-18 | 1999-11-16 | Delta Chemical Corporation | Polyaluminum chlorides and polyaluminum chlorosulfates methods and compositions |
US6174445B1 (en) | 1997-06-11 | 2001-01-16 | Br Technologies | Treatment of water with polynucleate metal hydroxide compounds |
US20050161339A1 (en) * | 2001-07-25 | 2005-07-28 | Haase Richard A. | Methods and processes for the manufacture of polynucleate metal compounds and disinfectants |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5337596A (en) * | 1976-09-20 | 1978-04-06 | Osaka Soda Co Ltd | Production of basic aluminium polychloride |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3113911A (en) * | 1960-09-06 | 1963-12-10 | Armour Pharma | Process of preparing aluminum chlorhydroxides and aluminum hydroxide |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB655617A (en) * | 1947-10-30 | 1951-07-25 | Peter Spence & Sons Ltd | Production of aqueous solutions of aluminium chloride |
DE1041933B (en) * | 1957-05-14 | 1958-10-30 | C F Asche & Co Ag | Process for the production of aluminum oxychloride |
JPS5137579B2 (en) * | 1972-06-16 | 1976-10-16 | ||
JPS50839A (en) * | 1973-04-28 | 1975-01-07 |
-
1972
- 1972-03-01 IT IT21252/72A patent/IT949756B/en active
-
1973
- 1973-02-22 ZA ZA731255A patent/ZA731255B/en unknown
- 1973-02-22 AU AU52476/73A patent/AU475570B2/en not_active Expired
- 1973-02-26 IE IE293/73A patent/IE37607B1/en unknown
- 1973-02-26 NO NO756/73A patent/NO131641C/no unknown
- 1973-02-26 BE BE795923D patent/BE795923A/en not_active IP Right Cessation
- 1973-02-26 CH CH279173A patent/CH560163A5/xx not_active IP Right Cessation
- 1973-02-27 TR TR17931A patent/TR17931A/en unknown
- 1973-02-27 RO RO7373990A patent/RO64459A/en unknown
- 1973-02-27 GB GB964773A patent/GB1410087A/en not_active Expired
- 1973-02-28 FR FR7307007A patent/FR2174114B1/fr not_active Expired
- 1973-02-28 DK DK110573A patent/DK143063C/en not_active IP Right Cessation
- 1973-02-28 DE DE2310014A patent/DE2310014C2/en not_active Expired
- 1973-02-28 IN IN448/CAL/73A patent/IN138595B/en unknown
- 1973-02-28 CS CS7300001443A patent/CS184813B2/en unknown
- 1973-02-28 HU HUSA2466A patent/HU165434B/hu unknown
- 1973-02-28 DD DD169660A patent/DD102370A5/xx unknown
- 1973-02-28 YU YU0531/73A patent/YU36664B/en unknown
- 1973-02-28 CA CA164,844A patent/CA1005969A/en not_active Expired
- 1973-02-28 ES ES412423A patent/ES412423A1/en not_active Expired
- 1973-02-28 LU LU67122D patent/LU67122A1/xx unknown
- 1973-02-28 NL NL7302847A patent/NL7302847A/xx unknown
- 1973-02-28 US US336753A patent/US3909439A/en not_active Expired - Lifetime
- 1973-03-01 AT AT182273A patent/AT329520B/en not_active IP Right Cessation
- 1973-03-01 AR AR246894A patent/AR201100A1/en active
- 1973-03-01 JP JP48023788A patent/JPS48101399A/ja active Pending
- 1973-03-01 ZM ZM32/73*UA patent/ZM3273A1/en unknown
- 1973-03-01 SE SE7302924A patent/SE388191B/en unknown
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3113911A (en) * | 1960-09-06 | 1963-12-10 | Armour Pharma | Process of preparing aluminum chlorhydroxides and aluminum hydroxide |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4082685A (en) * | 1974-03-28 | 1978-04-04 | Snamprogetti, S.P.A. | Process for the production of aluminum chlorohydroxides |
US5120522A (en) * | 1989-01-25 | 1992-06-09 | Caffaro S.P.A. | Process for preparing basic aluminum compounds |
US5182094A (en) * | 1989-02-13 | 1993-01-26 | Kemira Kemi Aktiebolag | Process for the preparation of polyaluminum compounds |
EP0554562A1 (en) * | 1992-02-01 | 1993-08-11 | A.I.R. Lippewerk Recycling GmbH | Process for the preparation of basic aluminium chloride solutions |
US5830388A (en) * | 1995-08-11 | 1998-11-03 | American Envirocare, Inc. | Coagulating and flocculating agent and method for making it |
US5985234A (en) * | 1995-09-18 | 1999-11-16 | Delta Chemical Corporation | Polyaluminum chlorides and polyaluminum chlorosulfates methods and compositions |
US5997838A (en) * | 1995-09-18 | 1999-12-07 | Delta Chemical Corporation | Polyaluminum chlorides and polyaluminum chlorosulfates methods and compositions |
US6036935A (en) * | 1995-09-18 | 2000-03-14 | Delta Chemical Corporation | Polyaluminum chlorides and polyaluminum chlorosulfates methods and compositions |
US6174445B1 (en) | 1997-06-11 | 2001-01-16 | Br Technologies | Treatment of water with polynucleate metal hydroxide compounds |
US20050161339A1 (en) * | 2001-07-25 | 2005-07-28 | Haase Richard A. | Methods and processes for the manufacture of polynucleate metal compounds and disinfectants |
Also Published As
Publication number | Publication date |
---|---|
CH560163A5 (en) | 1975-03-27 |
GB1410087A (en) | 1975-10-15 |
AT329520B (en) | 1976-05-10 |
IE37607L (en) | 1973-09-01 |
TR17931A (en) | 1976-11-01 |
NO131641C (en) | 1975-07-02 |
SE388191B (en) | 1976-09-27 |
ZM3273A1 (en) | 1974-02-21 |
CS184813B2 (en) | 1978-09-15 |
AU475570B2 (en) | 1976-08-26 |
DD102370A5 (en) | 1973-12-12 |
DK143063B (en) | 1981-03-23 |
ATA182273A (en) | 1975-08-15 |
NL7302847A (en) | 1973-09-04 |
DE2310014C2 (en) | 1982-08-26 |
RO64459A (en) | 1979-05-15 |
AU5247673A (en) | 1974-08-22 |
YU36664B (en) | 1984-08-31 |
LU67122A1 (en) | 1973-05-03 |
BE795923A (en) | 1973-06-18 |
FR2174114B1 (en) | 1976-06-11 |
JPS48101399A (en) | 1973-12-20 |
AR201100A1 (en) | 1975-02-14 |
IT949756B (en) | 1973-06-11 |
YU53173A (en) | 1981-11-13 |
IE37607B1 (en) | 1977-08-31 |
HU165434B (en) | 1974-08-28 |
ES412423A1 (en) | 1976-04-16 |
ZA731255B (en) | 1973-11-28 |
FR2174114A1 (en) | 1973-10-12 |
CA1005969A (en) | 1977-03-01 |
DE2310014A1 (en) | 1973-09-20 |
IN138595B (en) | 1976-02-28 |
NO131641B (en) | 1975-03-24 |
DK143063C (en) | 1981-11-02 |
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